Improvement in revivifying animal charcoal-for refining sugar



UNTTED STATES PATENT FlllCE.

.ABSALON H. LEPLAY ANI) .IULlUS F. J.ACU[SlN[ER, 0F PARS, FRANCE.

IMPROVEMENT IN REVIVIFYING ANIMAL CHARCOALFR REFINING SUGAR.

'Speeitiration forming part of Letters Patent No. 35,ll60, dated May 6, 1862.

To 11H whom, if 711/! 1/ erinnern:

lie it known that we, AHSALON HIPPOLYTE LEI-LAY :und .litmus lfRANtis JOSEPH tUIsr NIER, both ot' laris, in the l `renrh Empire,

have invented eertain new and useful improvement-s in revivityinn' blaek or rhareoal, in eolleetingl animoniaeal eases generati-d in the revivifieation, in the clarification of' saeeharine liquors, and in apparatus employed in the revivifieation ot the blaekand in the filtering ot'fsat-t-harine liquors; and we hereby det-lare the followingl to be a full, clear, and exact deseription ol the same, reference being had to the accompanving' drawings, in which- Figures l, 2, and Vli represent, respectively, a front elevation, part ly in section, a side elevation, and a plan view, of the apparatus hereinafter referred to and described.

Our invention consistsrst, in revivif'ying animal black or eharcoal b v wet processes,

hot water or steam acting in the. filtering-'t vessels, whether for renewing' its powers for absorbing lime or f'or renewing its properties for absorbingazotized,ammoniacal,and eolorlngl matters, as hereinafter described; second, 1an revlvifying animal blaek b vaeids to eliminate lime from deteeated saeeharine liquors,

as hereinafter described; third, in the elarii fieation of sapeharine liquors, juices, and sirups by means ot" phosphates, as hereinafter described; fourth,in theditterent methods of p eharine liquor is allowed to flow out through revivification of animal black, hereinafter described, which allow of' the collection of the ammoniaI given od in the revivification.

The object of our invention is to restore to the spent animal black its orignal properties and effect. its revivitiea-tion in the filter in which ithas been used.

\\'e have discovered that animal black possessies, first, the property of absorbing lime;

and second, the property of absorbing am mon iaeal, azotized, odorous, and coloring matters. j We have utilized these properties in the apl plication of our invention to saeeharine juices and sirups as follows:

XVe pla-ee the black in grains in the ordinary filter before introducing the sae-@hw rine liquor, juiee, or srup. We pass boiling Water through'it, orintrmluee steam to heat the black and td prevent the coloring of the saeeharine liquor to be acted on. lVeeha-rge l the filter with the juive or sirup, and the applieation of this process of revivitication only j commences some hours after the working of the filter, when the saceharine liquor ceases g to part with its eoloring,r property. It is-it'ound that at that moment the black has losta great portion of its properties for absorbing the azotized ammoniaeal odorous matters which are most injurious to crystallization and to the good qualities of ordinary sugar. If the operation be then suspended, it becomes easy to restore tothe black its primitive properfies. For this purpose filtration must be immediately stopped and the liquorin the filter must be allowed to run out. Then introduce at the lower part. of the filter a jet of steam, whieh penetrates through and between the grains of black. As soon as the steam reaches t the upper part of the filter there is given oft' a strong ammoniaeal odor, due to the ammo- I nia derived from the decomposition of the I organic azotized matters of.' the amlnoniaeal salts removed by the black from the sacchas rine liquor, The action of the steam is eon- I finned until the disengagement of the ainmoniaeal vapors ceases, generally from fifteen to thirty minutes, according; to the size of the f filter and the 'quantity of steam. The decomposition of these. matters and the dlisen gagement of the ammoniacal vapnrs may be faeilitated by adding on the filter a few quarts of a milk of lime at t-he time the sacthe bottom ot' the filter.

When closed filters are used, the milk of lime need not be added. A jet of steam may be introduced at the top of the tilt-er to ac- Celera-te the flowing' out of the saeeharine liquor and to prevent the 'access ot air to the filter. By this means, also, the time necessary for the revivification of the black is diminished. While this latter operation is going on portions of the steam become condensed on the bottom of the filter. This f condensed water is thick and contains sae charine and foreign matters. 'Ihis is drawn i ofi. and worked up with other impure pr ducts. As soon as this revivifying process is g complete the filtering of the saccharine liq- I uors is continued as long,r as the color is satisfactory and the limpidity of the liquor perfeet. Then the liquor ceases te possess these e 35,1 co

qualities, the black is re\'i\'ilicd, as before., economicalto collect' it an'd use it over again and this may be repeated live or six times, i for asimilar purpose. ln this state and withand even oltencr, in the same manner and with the same results. 'lhe revivilieation bel'ore described only restores to the black its )ro iertiesol'absorbingazotizcd ammoniacal oily, and coloring matters; lult when operatinguponsaeeharinemalterscontaininglimel as beet and eane juices-aller del'ecation it ol'ten happensthat al'lera certain time, aeeord- I substituted the one l'or the other, according ing to the quantity of .lime they contain, the

black loses its proprrtyol' absorbinglime, a-nd then it becomes indispensable to restore this property. 'lhc feed to the liller must befsuspended and vthe saceharine liquid therein must be allowed to run oli, and boiling water t mllst be introduced to eliminate the saeehaphuric acid and salts more or less acid-bull rine liquid with which the black is moistenerl.

'lhis elimination complete. lurther introduetion of boiling water is stopped and water:

aeidulated with hydrochloric acid, making:

I'rom three to six degrees by the areome'ter, is admitted; but the quantity ol` acid varies according to the quantity ot' lime absorbed by the blafek. 'lhe inlet of af-idula-ted water is stopped and freshwater admitted unt-il the oulllowing liquor reddens slightly, itl at all,

litmus-paper.

We t-hen entirely empty the 1 tilter et' liquid and leed again with the saeellarinelitpior. ll. will be understood thatby this last revivitication the deeoloring properproperty of absorbing lime and to render the re\'1\'1f\'1ng of this property less frequent, we :i

adopt the following means: 'l"he black we lound contains a small quantity of phosphate ot' lime, with two proportions ot' lime-that is to say, t-wo eqi'iivalents orprtniortions of lime to one equivalent or proportion of phosphoric acid. lt is to the presence ol' this phosphate that the black to a great extent owes its absorbing powers. In order to add to these powers t'or absorbing lime, we incorporate with it 'and increase the phosphate oit-lime, and this by placing the black in grains in contact with a solution of phosphate of lime with one proportion otlime. Instead of phosphate of lime we sometimes use phosphate of magnesia. 'lhe quantity of these phosphates capable of absorbing anew lime absorbed by the` black will depend upon the density of the solution ot the phosphate of' limo used to wet the black. Therefore' the property of animal black for absorbing lime may be increased or diminished at will by increasing or lessening the density of the solution placed in contact with the black and the time during which it is allowed so to remain. This operation should be perl'ormed in the filter, a sufficient quantity ol solution ot' phosphate of lime with one proportion oll lime to entirely cover the black being run into it. This solution is allowed to remain in contact with the black for some instants; then it is allowed to run out. lt is out l'urther 'prelmration or washing the filter is ready to be again used, and its use may be continued until one or otherol' the absorbing properties ol' the black, whether lor lime or l'or azotzed, ammoniaeal, odorous, and coloring' matters, be exhausted.

llither process l'or revivil'ying the properly ol' animal black lor absorbing lime may be to cireumslam-es: but when operating upon non-saturateddel'eeated juices the solublephosphate process is preferred.

Although we prefer hydrochloric acid in l he re\'i\il' ving process hereinbel'ore described` other acids may be employed-such,as sullheir action is less perfect. 'llle property ol' animal black lor absorbing lime will continue as long as the black retains the power of absorbing the solution ol' phosphate with one proportion ot lime; but should its power ol' absorbing azotized,ammoniaeal` and coloring matters become weak, notwithstandng the revivilicatzions ol' steam and milk. ot' lime, its primit ive properties may be restored by pouring upon it in the filter, a'l'ter by repeated \\'asl|ings it has been `t'reed from saecharine matter, a boiling solution olf carbonate ol' soda,.

or even eaustiesmla, olf l'rom three to six degrees density.v We allow the solution to remain in contact with the black for about an hour, and increase its energy, il'neeessary, by injecting a jet ot steam into the lower part of the filter until all trace ot amlnoi1iacal vapor disappears.y We allow the solution of soda to run otl",and inject steam to dispel all trace oll ammonia. We wash with water to remove all remains ofthe alkaline solution and apply vessel without recourse to ealcination isl thoroughly effected. Y

\Ve have stated these processes of reyivification may be carried on in ordinary filters. It will be suicient to add to the filters at the level of the under side of the false bottom perforated with holes a steam-cock, and to substitute for the cloth generally used on the false bottom a wire-gauze or metallic cloth,

.the meshes of which are sufficiently fine to' prevent the black passing through.

For the easy carrying of these processes into effect, the apparatus invented by us is of the construct-ion and rrangement shown in the aceompan ying drawings, in elevation,

During y at lfig. 2, und in plan at Fig.

. oovor kopt closo by svrows or bolts und nuts; t

(t, oook t'or trmptyi ng tho tiltor; si phon-oook;

j', portorn'tod i'itlso bottom oovorotl by motnllio oloth; g, si} il1on-} )ipo 'or tho outtlow ol' tho snochurint'e nutttor; 7i, (foil i'or sonding stwun into tho bottom oi?, tho tilt-or; i, steam-supply pipo; j, stomn-ootf'k for :ulmitting and shuttingo't't stonni into :ind i'roin tho coil; oook t'or :ulmittingstozlm into tho uppor purtot' tho liltor; l, num-holo t'or omptyiug tho blank; ni, recoivor of' tho tiltorod juii-,os or sirups; l', l sut'ot.\'\':1l\'o; o, pipo oommuniouting with :ill tho tiltors und loading tho gases through n l pipo, p, into :t sut'urttor. l l is tho snturator; u, rook for tho ontlot ot' t tho gusos t'rom tho tiltor; l] q, porforutztl dizli phragms tixod in tho shturntor; 1Q pipo t'or t lot t ing wutor into t ho suturnior; s, outlet-pipo t'rom sutnrutor; f, gus und vupor'ontlct pipo und rook; u, hir-cook. 'lho supply ol" mutter to be tiltorod, us also thoI stoom, may he udmittoil oithor :1t tho uppor or lower purt of tho tiltor.

ln tho (lrmvngs, :t tubo,.r, mlnfptod to ouch I iltor iXAJndiruti-s tho :irrirnl oi'juir(J :it tho I lowor pftrt of tho tltor.

'lho foregoing m'rungommit. ullows ot' tho introd1ution ut will olf strom. rlhov rlosod` tiltor also allows ot' dirof'ting und gathoriug tho ammonizuul Yztpors, whivh might also provoI injurious it ullowod to wirt-nlnto in tho i'zutory, in :i pipo plnood on tho top ol' tho? artly in soction at. Fig. l in sido .lo\\'ution 'iltor :1nd mudo to dip into vossols oontuin-i ing wzitor zu-idnlzitod with h'rdrochloriv or othor :li-id. ll.' ut'tor mnny slu'oossivo rvvivitit-.ntions by stwun tho liltrntion should boi i-omo slow, wo tuko out tho blntfk from ilul tiltor and thoroughly wzish il. ,lhen, without I t'urthor trontmont, roplnro it in tho tiltor.

Emploi/HAM o/"nnin/u/ Mdr/f [u pou-rtm1* 1 'lhis is Ohiotly nsod in tho rotining ot' sugur, vot troutod und nsod in thoso prooosses tor th(I uuuuitiu-tnro ot' sugur it nrquires inorcnsod iulportnnro. 'ilhtl umiliontionot' those provossos in ugrivnlturu-l dist-illorirs roquiros i n ronsidorubltl suppl)1 ot' \\:1tor,\\'hi(h the ugrit-nlturist muy not huw :1t (-onunnnd; and should ho proior usingl his blmk :is munuro, instoud ol' ro\'i\it' \'ing it` it will bo usol'ul to him to obtnin tho groutost :unouut possiblo t'rom tho absorbing und disvolorizing proportios otl thol blnvk. Now, by :i romploto trnnst'ornmtion ot tho lihu'li wo grontly inrrouso its powors ot' nbsorption` und :it thtl sumo time rodnt-o thtx pmnt it usi-d. 'Vhus we takotilnee pnrts ol' phosphuttl otlimo, with om1 proportion ot' limo` dissolw-il iu wnttu', :ind mix the solution with `linoly-powdorml :lnimnl blaik. 'lhi plio.-'.pliutix ol' linu` with throo-purts of; limo, whirh vonstilutos tho bnso ot' hnimnl black, is dostro \'id,ninl :i mixturo is l, tuin \fl `grohtor.

ot hor moans ol" nwoluu-iiuul sfpurution.

; sugur dosirod. ing prolu'wtios ot' th(l black have boon comcontaining phosphato with ono proportion of limo and phosphate with two proportions of limo. (This phosphate with two proportions of limo, whirh is insolnblo in wat-or, becomes solublol in n solution ot' phosphnto, wit-h ono proportion olf limo.) 'lho proportion of tho ono or tho othor muy bo inoroisod at will, :recording as it. is dosirod to inoronst, or liminish tho rolutivo quantity olf tho two (conlpositions. 'lho absorbing proporty for limo will bo :is mut-li grontor :is tho qunntityot phosphn-tol with ono proportion ot' limo is l.' this mixturo bo diluted with wittor, soztsto rondor it fluid, :ind it' it bopourod gradually und onutionsly on (lofoontod beet:-

jniro un abundantgolntinous precipitato will bo toi-mod on thobot-tom of tho vt'fssohonrryiug down with it tho black,` absorbing tho limo in tho juioo, und dot-oloriziug and clarifying the juice. This prof'ipitutois tho phosphate oi.' limo withthrooy proportions oi' limo, whioh possossos tho proportr ot.l pwripituting itself in :i golnt inous torni, whith rontributos to thotflziritioution ot' tho ,iuior to th(l separation ol the t black nndot' nil tho mnttors in suspension in :i

romzlrlmblo munnor. It' tho addition oi this semi-fluid mixturobo coutinuod and tho. 'miro tur@v bo woll stirred into tho juico, tho lzittor will soon loso the wholo or tho grontor part.

of its alkalinity,whit-h is useorta-inod bytesting with litmus-paper, und the rosult will be u f dooolorizod and flnritied juiro treo, or nearly so, of limo. rlhisoporation should tukoplare upon th(l (flour iuioo :is soon as it homos out ot tho dot'omtingwossol. It doos not rf-quiro rohoziting. After having bron treated uslast dosvribod tho juito is'ullowod to sottlo some` minutos und thon drown ott' (door. Tho doposit is roet-iwd in u tiltor, or nndorgoes The juioo thus tilt-rod muy bo baked directly, or it muy bo passed through animal black. in u granular stato, nffording to thel qualityof Tho nbsorbingmul docolorizpit-duly oxhnustod, and it may thon lie advri-nt-ugmmsl)Y used as nmnurt-f. It muy bo utilizod in tho preparation ot phosphate ot limo, with one proportion of lime, after hm'- ing beou rultiuod in tho openair. Ewen in @use ot' nood it muy bo rogenorated by boiling it with u` solution of caustic soda, and zitter sovornl washings revivit'ying it by the solution ot' phosphnto with ono'proportion of limo. 4

(ivlci/i/if'u/[ou (.g/'sllm'm/'nf' Holm/'s in .suf/m houses, uml pur/iruor/vf/ u rqium'es.'l`he golatinous lwooipitnto, horoiulwtoroY referred to, with :t baso ot' phospluito with t-ln'eol proportions ot' limo, when added t-o :i snoolmrine liquor containing limo, talios the place, and we nso it instead of, ulbumou and blood, gen erallv nsod in sugar-retinfn'ios. howevor, bo .tnkon not to usol it in excess. 'lljw blzu'k hns :L very not'ivo decolorizing :w-

wliioh it is used.

(lure must,

' the ordinary manner.

' down tho black in precipitating;

` phosphatel is suic'ent, thc whole is carl-imi to the.boiling-point, skimmed, and filtered in lhe Aphosplmte with one proportion ol' linieI inn-y be prolmrcd by burning nt n whitel honi. the LLnimnl block in contact with, the nir. nnd by fronting tho cai-lcincd .pro 'luct with two proportions olf sulphuric heid. 'lho phospho-to with-three proportions o1.' linie becomes destroyed, two proportions of sulplmd'o of limo become formed und :preeipi`t'\.ted, :und oneproportion Yroumains:

in solution. vThis solution may he employed :is it is, or il nmybo concentrated 1o eliminate n little of the sulphate of' lime. We somotimos preparo the solublcphoSphn-tc withonc prmmrtion of linie with nnimnl black in groin or in powder by adding the snmo quantity of sulphur-ic acid. 'lhc sulphate of lime carries l The phos-l phate of liniel rcnmins still with one proporlion of linie, :und is dissolved. y l

Hoving thus fully described our invent-ifm, we shall state our claims, :is follows:

chnrine liquors, juices, and Srups by means of phosphates, substantially :is hereinbefore Sc-t forth.

Si. 'lhe manner of operating und effecting, by moans of the diiierent processes described;

the rcvivificntion of animal black or charcoal, so :is to allow of the collection of the ammonin given off in the revivificntion.

In testimony whereof we have signed our names to this specification before two subv scribing witnesses.

A. H. LEPLAY. J. F. J. oUIsINIER.

Witnessee:A GEO. IIU'r'roN, L. CLAR. 

